Triethylamine → 2-(Chloromethyl)-5-(4-(trifluoromethyl)phenyl)thiophene

HRID 1785218

反応式

HRID 1785218 の反応式
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][C:6]([C:9]2[S:13][C:12]([CH2:14]O)=[CH:11][CH:10]=2)=[CH:5][CH:4]=1.C(N(CC)CC)C.CS([Cl:29])(=O)=O>C(Cl)Cl>[Cl:29][CH2:14][C:12]1[S:13][C:9]([C:6]2[CH:7]=[CH:8][C:3]([C:2]([F:17])([F:16])[F:1])=[CH:4][CH:5]=2)=[CH:10][CH:11]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 219863522-Thiophenemethanol, 5-[4-(trifluoromethyl)phenyl]-

生成物 1

HCID 575949792-(Chloromethyl)-5-(4-(trifluoromethyl)phenyl)thiophene

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a mixture of [5-(4-Trifluoromethyl-phenyl)-thiophen-2-yl]-methanol (1.52 g, 5.89 mmole) and triethyl amine (1.64 mL, 11.78 mmole) in DCM (100 mL) at 0° C., is injected methanesulfonyl chloride (0.91 mL, 11.78 mmole) dropwise. The reaction is kept at 0° C. for an hour and warmed up to room temperature for an hour. The reaction mixture is concentrated on rota vapor, and the resulting residue is purified on a silica gel column, eluting with 0-15% ethyl acetate in hexane and concentrated to provide the titled compound as off-white solid.

後処理

  1. waitThe reaction is kept at 0° C. for an hour
  2. concentrationThe reaction mixture is concentrated on rota vapor
  3. customthe resulting residue is purified on a silica gel column
  4. washeluting with 0-15% ethyl acetate in hexane
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-98d68cde2bec498d802059a64c64ffde
出典データセット
uspto-grants-2009_03
特許番号
US07504433B2

関連ノート

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